#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/30/4323039.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323039
loop_
_publ_author_name
'Fernando Canales'
'M. Concepción Gimeno'
'Antonio Laguna'
_publ_section_title
;
 Heterobimetallic Complexes of Gold(I) with the Tetrathiovanadate Anion.
 Crystal Structure of [VS4(AuPPh3)2{Au(PPh3)2}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5376
_journal_page_last               5379
_journal_paper_doi               10.1021/ic9712939
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C72 H60 Au3 P4 S4 V'
_chemical_formula_weight         1819.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 129.466(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.110(6)
_cell_length_b                   13.087(2)
_cell_length_c                   20.620(3)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      3
_cell_volume                     6689(2)
_computing_cell_refinement       Siemens-XSCANS
_computing_data_collection       Siemens-XSCANS
_computing_data_reduction        Siemens-XSCANS
_computing_molecular_graphics    Siemens-XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       Siemens-P4
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8076
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.836
_refine_ls_goodness_of_fit_obs   0.982
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.914
_refine_ls_restrained_S_obs      0.932
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_obs          0.0399
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0133P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0814
_refine_ls_wR_factor_obs         0.0662
_reflns_number_observed          2595
_reflns_number_total             4097
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9712939.cif
_cod_data_source_block           concha4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (20 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (47
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy-atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        6689.4(19)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4323039
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Au1 Au 0.10090(2) 0.04683(4) 0.78473(3) 0.0258(2) Uani 1 d . .
Au2 Au 0.0000 0.27195(5) 0.7500 0.0217(2) Uani 1 d S .
V V 0.0000 0.0401(2) 0.7500 0.0184(7) Uani 1 d S .
S1 S 0.07168(10) 0.1364(2) 0.8495(2) 0.0209(8) Uani 1 d . .
S2 S 0.01717(11) -0.0546(2) 0.6848(2) 0.0303(9) Uani 1 d . .
P1 P 0.17023(11) 0.0189(2) 0.7838(2) 0.0212(8) Uani 1 d . .
P2 P -0.00787(11) 0.3595(2) 0.8417(2) 0.0212(8) Uani 1 d . .
C11 C 0.1495(4) 0.0320(8) 0.6779(8) 0.027(3) Uani 1 d DU .
C12 C 0.1150(4) 0.1111(8) 0.6294(8) 0.032(3) Uani 1 d DU .
H12 H 0.1033(4) 0.1541(8) 0.6522(8) 0.039 Uiso 1 calc R .
C13 C 0.0970(4) 0.1306(9) 0.5516(8) 0.037(3) Uani 1 d DU .
H13 H 0.0724(4) 0.1849(9) 0.5194(8) 0.044 Uiso 1 calc R .
C14 C 0.1156(4) 0.0681(8) 0.5187(9) 0.037(3) Uani 1 d DU .
H14 H 0.1038(4) 0.0810(8) 0.4640(9) 0.044 Uiso 1 calc R .
C15 C 0.1512(5) -0.0127(9) 0.5661(8) 0.037(3) Uani 1 d DU .
H15 H 0.1641(5) -0.0547(9) 0.5447(8) 0.044 Uiso 1 calc R .
C16 C 0.1667(4) -0.0290(9) 0.6437(8) 0.027(3) Uani 1 d DU .
H16 H 0.1904(4) -0.0844(9) 0.6760(8) 0.033 Uiso 1 calc R .
C21 C 0.2292(4) 0.1043(8) 0.8480(7) 0.021(3) Uani 1 d DU .
C22 C 0.2561(4) 0.1361(8) 0.8181(7) 0.030(3) Uani 1 d DU .
H22 H 0.2426(4) 0.1167(8) 0.7634(7) 0.037 Uiso 1 calc R .
C23 C 0.3024(4) 0.1958(8) 0.8683(8) 0.034(3) Uani 1 d DU .
H23 H 0.3209(4) 0.2177(8) 0.8488(8) 0.041 Uiso 1 calc R .
C24 C 0.3208(5) 0.2226(9) 0.9484(8) 0.041(3) Uani 1 d DU .
H24 H 0.3521(5) 0.2640(9) 0.9832(8) 0.049 Uiso 1 calc R .
C25 C 0.2950(5) 0.1907(9) 0.9782(8) 0.041(3) Uani 1 d DU .
H25 H 0.3085(5) 0.2087(9) 1.0331(8) 0.049 Uiso 1 calc R .
C26 C 0.2491(4) 0.1322(9) 0.9266(8) 0.032(3) Uani 1 d DU .
H26 H 0.2307(4) 0.1108(9) 0.9465(8) 0.038 Uiso 1 calc R .
C31 C 0.1994(4) -0.1091(9) 0.8230(7) 0.024(3) Uani 1 d DU .
C32 C 0.1690(4) -0.1853(8) 0.8212(7) 0.025(3) Uani 1 d DU .
H32 H 0.1338(4) -0.1703(8) 0.8021(7) 0.030 Uiso 1 calc R .
C33 C 0.1893(5) -0.2838(9) 0.8470(8) 0.043(3) Uani 1 d DU .
H33 H 0.1676(5) -0.3359(9) 0.8443(8) 0.052 Uiso 1 calc R .
C34 C 0.2404(5) -0.3067(10) 0.8765(9) 0.049(4) Uani 1 d DU .
H34 H 0.2546(5) -0.3735(10) 0.8965(9) 0.059 Uiso 1 calc R .
C35 C 0.2713(5) -0.2319(9) 0.8768(9) 0.049(4) Uani 1 d DU .
H35 H 0.3060(5) -0.2481(9) 0.8944(9) 0.059 Uiso 1 calc R .
C36 C 0.2510(4) -0.1327(9) 0.8511(8) 0.038(3) Uani 1 d DU .
H36 H 0.2724(4) -0.0810(9) 0.8528(8) 0.046 Uiso 1 calc R .
C41 C -0.0767(4) 0.3842(8) 0.8037(7) 0.027(3) Uani 1 d DU .
C42 C -0.1194(5) 0.3800(10) 0.7179(9) 0.056(4) Uani 1 d DU .
H42 H -0.1132(5) 0.3636(10) 0.6798(9) 0.067 Uiso 1 calc R .
C43 C -0.1725(5) 0.4004(12) 0.6879(10) 0.078(5) Uani 1 d DU .
H43 H -0.2019(5) 0.4006(12) 0.6293(10) 0.093 Uiso 1 calc R .
C44 C -0.1810(5) 0.4197(11) 0.7432(9) 0.058(4) Uani 1 d DU .
H44 H -0.2169(5) 0.4305(11) 0.7222(9) 0.070 Uiso 1 calc R .
C45 C -0.1402(5) 0.4241(10) 0.8273(10) 0.054(4) Uani 1 d DU .
H45 H -0.1472(5) 0.4390(10) 0.8647(10) 0.064 Uiso 1 calc R .
C46 C -0.0862(4) 0.4057(10) 0.8582(9) 0.040(3) Uani 1 d DU .
H46 H -0.0570(4) 0.4084(10) 0.9169(9) 0.048 Uiso 1 calc R .
C51 C 0.0228(4) 0.4839(8) 0.8638(8) 0.036(3) Uani 1 d DU .
C52 C 0.0785(5) 0.4877(9) 0.9086(8) 0.044(4) Uani 1 d DU .
H52 H 0.0985(5) 0.4257(9) 0.9282(8) 0.052 Uiso 1 calc R .
C53 C 0.1058(5) 0.5798(10) 0.9254(9) 0.059(4) Uani 1 d DU .
H53 H 0.1437(5) 0.5805(10) 0.9562(9) 0.070 Uiso 1 calc R .
C54 C 0.0769(5) 0.6694(10) 0.8966(10) 0.068(5) Uani 1 d DU .
H54 H 0.0951(5) 0.7323(10) 0.9079(10) 0.081 Uiso 1 calc R .
C55 C 0.0212(6) 0.6696(9) 0.8511(12) 0.074(5) Uani 1 d DU .
H55 H 0.0012(6) 0.7314(9) 0.8309(12) 0.089 Uiso 1 calc R .
C56 C -0.0041(6) 0.5751(9) 0.8362(11) 0.066(5) Uani 1 d DU .
H56 H -0.0420(6) 0.5744(9) 0.8052(11) 0.079 Uiso 1 calc R .
C61 C 0.0241(4) 0.3017(7) 0.9437(8) 0.024(3) Uani 1 d DU .
C62 C 0.0514(5) 0.3563(9) 1.0183(8) 0.031(3) Uani 1 d DU .
H62 H 0.0552(5) 0.4282(9) 1.0175(8) 0.037 Uiso 1 calc R .
C63 C 0.0735(5) 0.3081(10) 1.0944(8) 0.039(3) Uani 1 d DU .
H63 H 0.0939(5) 0.3456(10) 1.1455(8) 0.047 Uiso 1 calc R .
C64 C 0.0651(4) 0.2055(9) 1.0934(9) 0.035(3) Uani 1 d DU .
H64 H 0.0780(4) 0.1728(9) 1.1442(9) 0.041 Uiso 1 calc R .
C65 C 0.0387(5) 0.1485(9) 1.0216(8) 0.029(3) Uani 1 d DU .
H65 H 0.0341(5) 0.0771(9) 1.0233(8) 0.035 Uiso 1 calc R .
C66 C 0.0187(4) 0.1954(8) 0.9466(8) 0.026(3) Uani 1 d DU .
H66 H 0.0012(4) 0.1556(8) 0.8969(8) 0.031 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 S1 145.66(11) . . y
P1 Au1 S2 117.18(11) . . y
S1 Au1 S2 97.11(9) . . y
P1 Au1 V 164.00(9) . . y
S1 Au1 V 50.33(8) . . y
S2 Au1 V 46.82(8) . . y
P2 Au2 P2 121.8(2) . 2_556 y
P2 Au2 S1 118.44(10) . 2_556 y
P2 Au2 S1 101.10(11) 2_556 2_556 y
P2 Au2 S1 101.10(10) . . y
P2 Au2 S1 118.44(10) 2_556 . y
S1 Au2 S1 93.10(13) 2_556 . y
P2 Au2 V 119.09(8) . . y
P2 Au2 V 119.09(8) 2_556 . y
S1 Au2 V 46.55(6) 2_556 . y
S1 Au2 V 46.55(6) . . y
S2 V S2 109.3(2) 2_556 . y
S2 V S1 105.85(12) 2_556 . y
S2 V S1 111.93(10) . . y
S2 V S1 111.93(10) 2_556 2_556 y
S2 V S1 105.85(12) . 2_556 y
S1 V S1 112.1(2) . 2_556 y
S2 V Au1 57.92(7) 2_556 2_556 y
S2 V Au1 124.53(10) . 2_556 y
S1 V Au1 123.53(10) . 2_556 y
S1 V Au1 54.06(7) 2_556 2_556 y
S2 V Au1 124.53(10) 2_556 . y
S2 V Au1 57.92(8) . . y
S1 V Au1 54.06(7) . . y
S1 V Au1 123.53(10) 2_556 . y
Au1 V Au1 176.45(11) 2_556 . y
S2 V Au2 125.37(11) 2_556 . y
S2 V Au2 125.37(11) . . y
S1 V Au2 56.04(9) . . y
S1 V Au2 56.04(9) 2_556 . y
Au1 V Au2 88.23(6) 2_556 . y
Au1 V Au2 88.23(6) . . y
V S1 Au1 75.62(10) . . y
V S1 Au2 77.40(10) . . y
Au1 S1 Au2 111.33(13) . . y
V S2 Au1 75.25(10) . . y
C31 P1 C11 107.8(5) . . ?
C31 P1 C21 103.4(5) . . ?
C11 P1 C21 103.2(5) . . ?
C31 P1 Au1 111.8(3) . . y
C11 P1 Au1 112.2(3) . . y
C21 P1 Au1 117.5(3) . . y
C51 P2 C61 105.5(5) . . ?
C51 P2 C41 105.3(5) . . ?
C61 P2 C41 101.9(5) . . ?
C51 P2 Au2 108.8(4) . . y
C61 P2 Au2 117.1(3) . . y
C41 P2 Au2 117.1(4) . . y
C12 C11 C16 117.3(12) . . ?
C12 C11 P1 116.7(9) . . ?
C16 C11 P1 126.0(9) . . ?
C13 C12 C11 123.3(12) . . ?
C12 C13 C14 118.1(12) . . ?
C15 C14 C13 120.6(13) . . ?
C16 C15 C14 117.8(12) . . ?
C15 C16 C11 122.8(11) . . ?
C26 C21 C22 119.4(11) . . ?
C26 C21 P1 120.5(8) . . ?
C22 C21 P1 120.0(9) . . ?
C23 C22 C21 120.2(11) . . ?
C22 C23 C24 118.0(11) . . ?
C25 C24 C23 122.0(12) . . ?
C24 C25 C26 118.6(12) . . ?
C21 C26 C25 121.9(11) . . ?
C32 C31 C36 118.9(11) . . ?
C32 C31 P1 119.5(8) . . ?
C36 C31 P1 121.6(8) . . ?
C31 C32 C33 120.5(10) . . ?
C34 C33 C32 120.7(12) . . ?
C33 C34 C35 119.8(13) . . ?
C34 C35 C36 119.4(11) . . ?
C31 C36 C35 120.6(11) . . ?
C46 C41 C42 120.0(11) . . ?
C46 C41 P2 121.4(9) . . ?
C42 C41 P2 118.6(9) . . ?
C41 C42 C43 119.1(13) . . ?
C44 C43 C42 119.7(14) . . ?
C43 C44 C45 122.5(13) . . ?
C44 C45 C46 118.2(13) . . ?
C41 C46 C45 120.4(12) . . ?
C56 C51 C52 116.7(12) . . ?
C56 C51 P2 125.7(9) . . ?
C52 C51 P2 117.5(8) . . ?
C53 C52 C51 122.0(12) . . ?
C54 C53 C52 118.9(12) . . ?
C53 C54 C55 121.2(13) . . ?
C54 C55 C56 117.5(13) . . ?
C51 C56 C55 123.6(12) . . ?
C62 C61 C66 118.0(12) . . ?
C62 C61 P2 124.1(9) . . ?
C66 C61 P2 117.8(9) . . ?
C61 C62 C63 121.6(12) . . ?
C64 C63 C62 118.2(12) . . ?
C63 C64 C65 122.2(13) . . ?
C64 C65 C66 119.7(11) . . ?
C65 C66 C61 120.2(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.268(3) . y
Au1 S1 2.374(3) . y
Au1 S2 2.489(3) . y
Au1 V 2.8405(7) . y
Au2 P2 2.358(3) . y
Au2 P2 2.358(3) 2_556 y
Au2 S1 2.579(3) 2_556 y
Au2 S1 2.579(3) . y
Au2 V 3.034(3) . y
V S2 2.142(3) 2_556 y
V S2 2.142(3) . y
V S1 2.257(3) . y
V S1 2.257(3) 2_556 y
V Au1 2.8405(7) 2_556 y
P1 C31 1.837(12) . y
P1 C11 1.840(13) . y
P1 C21 1.845(11) . y
P2 C51 1.805(11) . y
P2 C61 1.818(13) . y
P2 C41 1.846(11) . y
C11 C12 1.376(13) . ?
C11 C16 1.393(13) . ?
C12 C13 1.339(15) . ?
C13 C14 1.415(14) . ?
C14 C15 1.400(13) . ?
C15 C16 1.356(14) . ?
C21 C26 1.362(14) . ?
C21 C22 1.406(13) . ?
C22 C23 1.391(13) . ?
C23 C24 1.400(15) . ?
C24 C25 1.372(14) . ?
C25 C26 1.378(13) . ?
C31 C32 1.381(13) . ?
C31 C36 1.397(12) . ?
C32 C33 1.389(13) . ?
C33 C34 1.371(13) . ?
C34 C35 1.392(14) . ?
C35 C36 1.397(14) . ?
C41 C46 1.368(14) . ?
C41 C42 1.388(14) . ?
C42 C43 1.422(14) . ?
C43 C44 1.35(2) . ?
C44 C45 1.36(2) . ?
C45 C46 1.436(14) . ?
C51 C56 1.366(14) . ?
C51 C52 1.400(13) . ?
C52 C53 1.398(14) . ?
C53 C54 1.374(15) . ?
C54 C55 1.39(2) . ?
C55 C56 1.403(14) . ?
C61 C62 1.391(14) . ?
C61 C66 1.408(13) . ?
C62 C63 1.40(2) . ?
C63 C64 1.367(14) . ?
C64 C65 1.367(14) . ?
C65 C66 1.385(14) . ?
